<blockquote><p><i>Anna Lenartowicz (1); Julia Mironenka (1); Adrian Soboń (1,2); Rafał Szewczyk (1,2); Katarzyna Krupczyńska-Stopa (1,2); Maciej Stopa (1,2); Andrzej Kwaśnica (3)</i><br><i>1 – LabExperts sp. z o. o., Gdańsk, Poland; 2 – </i><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/companies/315"><i><strong>Bioanalytic</strong></i></a><i> sp. z o. o., Gdańsk, Poland; 3 – Lab4Tox sp. z o. o., Wrocław, Poland</i></p></blockquote><h4><strong>Introduction</strong></h4><p>Compound presence confirmation is one of the key aspects of targeted and quantitative analysis in forensics applications. High resolution tandem mass spectrometry (HR-MS/MS) may become a major tool for this kind of analysis because of its mass accuracy resulting in unparallel specificity, all combined with broad linearity and scanning speed achieved in the newest hardware on the market. In this work we show a modern HR-MS/MS method for a sensitive detection of 27 analytes with high confidence in venous blood and blood collected on a volumetric absorptive microsampling (VAMS) probe. Analytes include: Tramadol, Morphine, Fentanyl, Methadone, Codeine, Alprazolam, Diazepam, Flunitrazepam, Lorazepam, Oxazepam, Zolpiclone, Clonazepam, Nordiazepam, Zolpidem, Hydroxyzine, Amphetamine, Methamphetamine, MDA, MDMA, MDEA, THC, Cocaine, 6-acetylmorphine, 7-aminoflunitrazepam, 7-aminoclonazepam, Benzoylecgonine, THC-COOH.</p><h4><strong>Materials and Methods</strong></h4><p>Briefly, sample preparation included: spiking of internal standards, protein precipitation and extraction using acetonitrile:methanol (1:1) with 0.1% formic acid, evaporation under nitrogen stream and reconstitution in LC mobile phase. Compounds were analyzed using reversed-phase chromatography on ExionAC LC coupled with ZenoTOF 7600 (SCIEX) operating in positive electrospray ionization scheduled MRMhr mode acquiring full MS/MS spectra for each compound. Developed processing method use multi-level confirmation and combined scoring based on HR data where result is affected by 5 criteria that have different decision weights: MS/MS library confirmation (50%), precursor ion mass defect (20%), quantifier ion mass defect (20%), precursor ion isotope pattern (5%) and retention time (5%). Each criterium contributes in the combined score calculation and has its own range of 3-level acceptance in ppm, % or seconds, respectively. The cut-off point of combined score is estimated at 70% after series of analysis and allows flawless reporting of compounds from DRUID list. Data were processed in SCIEX OS software.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Bioanalytics_Figure_1_Procedure_of_blood_samples_preparation_ed1d01bbb3.jpg" alt="Bioanalytics: Figure 1. Procedure of blood samples preparation." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Bioanalytics_Figure_1_Procedure_of_blood_samples_preparation_ed1d01bbb3.jpg 167w," sizes="100vw" width="1256" height="1177"></p><h4><strong>Results</strong></h4><p>The method was validated separately for blood and blood collected on VAMS and fulfilled the following criteria for each analyte: linearity (R ≥ 0.995), working range (LLOQ – 50 ng/ml), reproducibility (%CV ≤ 15%), accuracy (80 – 120%) and recovery (80 – 120%). For majority of analytes included in the method LLOQ was in the range 0.01- 0.05 ng/ml (ex. Diazepam, Flunitrazepam, Kodeine, Morphine, MDA) for blood and 0.05-0.1 ng/ml for VAMS sampler. For analytes such as Tramadol, Fentanyl, Methadone and Cocaine the LLOQ ranged between 0.001- 0.005 ng/ml for blood and 0.01-0.05 for VAMS. The method was successfully applied to routine analysis of blood samples.</p><p><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Bioanalytics_Table_1_Parameters_applied_in_LC_MS_MS_method_a71f5fed46.jpg" alt="Bioanalytics: Table 1. Parameters applied in LC-MS_MS method" srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Bioanalytics_Table_1_Parameters_applied_in_LC_MS_MS_method_a71f5fed46.jpg 245w," sizes="100vw" width="1162" height="323"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Bioanalytics_Figure_2_Chromatogram_presenting_LC_MS_MS_analysis_of_27_psychoactiv_compounds_from_DRUID_list_b369671a31.jpg" alt="Bioanalytics: Figure 2. Chromatogram presenting LC-MS_MS analysis of 27 psychoactiv compounds from DRUID list." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Bioanalytics_Figure_2_Chromatogram_presenting_LC_MS_MS_analysis_of_27_psychoactiv_compounds_from_DRUID_list_b369671a31.jpg 245w," sizes="100vw" width="1884" height="753"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Bioanalytics_Figure_3_Criteria_applied_in_developed_processing_method_using_a_multi_level_confirmation_and_combined_scoring_based_on_HR_data_e6f93aa598.jpg" alt="Bioanalytics: Figure 3. Criteria applied in developed processing method using a multi-level confirmation and combined scoring based on HR data." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Bioanalytics_Figure_3_Criteria_applied_in_developed_processing_method_using_a_multi_level_confirmation_and_combined_scoring_based_on_HR_data_e6f93aa598.jpg 245w," sizes="100vw" width="1893" height="1060"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Bioanalytics_Table_2_Results_of_quantitative_methods_validation_74781e6dcf.jpg" alt="Bioanalytics: Table 2. Results of quantitative methods validation." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Bioanalytics_Table_2_Results_of_quantitative_methods_validation_74781e6dcf.jpg 162w," sizes="100vw" width="1162" height="1120"><img src="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/Bioanalytics_Figure_4_Example_of_false_positive_result_exclusion_for_Metamphetamine_in_unspiked_venous_blood_sample_due_to_multi_level_confirmation_method_cd0fc2540a.jpg" alt="Bioanalytics: Figure 4. Example of false positive result exclusion for Metamphetamine in unspiked venous blood sample due to multi-level confirmation method." srcset="https://storage.googleapis.com/labrulez-bucket-strapi-h3hsga3/thumbnail_Bioanalytics_Figure_4_Example_of_false_positive_result_exclusion_for_Metamphetamine_in_unspiked_venous_blood_sample_due_to_multi_level_confirmation_method_cd0fc2540a.jpg 147w," sizes="100vw" width="1173" height="1246"></p><h4><strong>Discussions and Conclusions</strong></h4><p>A quantitative LC-MS/MS method was validated according to the international recommendations. The greatest advantage of presented method is its high specificity and extremely low Limits of Quantitation. Most of described in literature LC-MS/MS methods used for psychoactive compounds quantification are based on MRM scanning mode with triple quadrupole instruments. Such approach does not allow to obtain sufficiently high specificity because of difficult data interpretation at low concentrations of analytes in real-life samples where MRM ratio and matrix interferences leads to data misinterpretation. Developed method allows sensitive, specific and false positive resistant HR-MS/MS quantitation of 27 psychoactive compounds in blood and blood collected by VAMS.</p>

How sure you can be of the results of quantification of psychoactive compounds in blood?

News from LabRulezLCMS Library - Week 14, 2025

News from LabRulezLCMS Library - Week 19, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 30th June 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you other document by <strong>Agilent Technologies </strong>and posters by<strong> Shimadzu / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS!</strong></p><h3><strong>1. Agilent Technologies: Agilent InfinityLab Assist Hub: Representing Advancements in Cybersecurity</strong></h3><ul><li>Other document (white paper)</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/wp_infinitylab_assist_cybersecurity_5994_8261en_agilent_310c5c9a6c.pdf"><strong>Full PDF for download</strong></a></li></ul><h4><strong>The laboratory as an operational technology (OT) environment: bridging the gap between OT and IT&nbsp;</strong></h4><p>Compared to connected industrial production environments, the connected laboratory environment closely aligns with an operational technology (OT) environment. OT is defined as "the practice of using hardware and software to control industrial equipment, and it primarily interacts with the physical world" (RedHAT, 2024).&nbsp;</p><p>In the classical Purdue reference model, established in the early 1990s to protect identities, information, and assets, the OT environment is clearly separated and secured from the information technology (IT)/enterprise environment.&nbsp;</p><p>The model only allows direct communication between adjacent levels. OT environments (lab environments) are necessary due to the long life cycles of the systems typically exposed to cybersecurity threats, with the mitigations listed in Table 1.&nbsp;</p><p>Addressing cybersecurity challenges in OT environments requires customized security strategies that incorporate both traditional IT security principles and specific measures for the physical operations they control.&nbsp;</p><p>Unlike some IT system components and devices where complete infrastructure replacement is common, lab devices are typically replaced gradually over years, sometimes even over&nbsp;decades.</p><p>The clear separation between OT and IT is becoming increasingly blurred due to new connectivity requirements, cloud functionality, and Industrial Internet of Things integration. This process, known as IT/OT convergence, is essential for achieving the next level of automation, such as Industry 4.0/5.0 or its counterparts, such as Pharma 4.0. The effectiveness of any new development will be evaluated based on how well it addresses cybersecurity within a converging IT/OT environment.</p><h4><strong>Standards and organizations&nbsp;</strong></h4><p>The diverse standards and organizations can be exemplified by the approaches taken in the U.S., Europe, and China. This summary aims to showcase the complexity of regulatory environments, and is not comprehensive. For specific situations, consulting with dedicated field experts is crucial.</p><h5><strong>Europe&nbsp;</strong></h5><p>European cybersecurity regulations prioritize privacy and data protection, with an emphasis on harmonizing standards across member states.&nbsp;</p><ul><li><strong>General Data Protection Regulation (GDPR): </strong>GDPR is the cornerstone of data protection in the European Union (EU). It sets strict rules on handling personal data, including requirements for data breach notifications, data minimization, and individual rights over personal data. Noncompliance can result in severe fines.</li><li><strong>Network and Information Security Directive (NIS&nbsp;Directive): </strong>Adopted in 2016, the NIS Directive focuses on the cybersecurity of essential services (such as energy, transportation, and finance) and digital service providers. It requires member states to strengthen their national cybersecurity capabilities and cooperation.&nbsp;</li><li><strong>European Union Agency for Cybersecurity (ENISA):</strong> ENISA is the EU's dedicated cybersecurity agency, helping to develop and promote cybersecurity standards across Europe, including guidelines for incident reporting and cybersecurity&nbsp;certifications.</li><li><strong>ISO/IEC 27001: </strong>While ISO/IEC 27001 is a global standard for information security management systems, it is heavily adopted in Europe. This standard outlines processes for systematically managing sensitive company information, ensuring its security.&nbsp;</li><li><strong>Cybersecurity Act (EU): </strong>The Cybersecurity Act establishes a framework for cybersecurity certification for products, services, and processes, ensuring they meet recognized EU-wide standards.</li></ul><h4><strong>Conclusion&nbsp;</strong></h4><p>With the initial release of the InfinityLab Assist Control Software, the InfinityLab Assist Hub offers plenty of cybersecurity features that can be leveraged for a secure lab network environment founded on a customer-specific OT/IT security strategy.</p><h3><strong>2. Shimadzu / ASMS: Single Quadrupole Mass Spectrometry Quick Workflows Specified to Oligonucleotides Screening&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_TP_605_fa8deb906e.pdf"><strong>Full PDF for download</strong></a></li></ul><p>A workflow has been developed to deliver molecular mass information on the full-length product and related impurities for chemically synthesized oligonucleotides by applying a deconvolution algorithm to all detected components within a targeted data stream (UV/PDA, TIC or BPC). It has been designed to simplify the data processing experience without the need for a sequence input delivering results quickly by automating mass assignment of all detected components in a data stream.</p><h4><strong>2. Materials and Methods&nbsp;</strong></h4><h5><strong>2.1 LC-MS/MS method&nbsp;</strong></h5><p><strong>20-mer sample.</strong> A phosphorothioate-modified oligonucleotide purified was used as a model sample (20-mer anti-sense oligo; C229 H316 N69 O121 P19 S19; average mass 7168.05, Te-smCe-sTe-sTe-sGe-sGd-sTd-sTd-sAd-sCd-sAd-sTd-sGd-sAd-sAd-sAe-sTe-smCe-smCesmCe) spiked with 10% impurities (N-1(5’) and N-3(5’) shortmers) to the full-length product.&nbsp;</p><p><strong>80-mer antisense DNA sample</strong>. 80-mer PolyT oligonucleotide sample (C800 H1041 N160 O558 P79; average mass 24273.62) was also analyzed was analyzed by ion-pair reversedphase chromatography mode using HFIP (hexafluoroisopropanol) and 10 mM TEA (triethylamine).</p><p><strong>LC Separation</strong>. Components were separated using the Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=Nexera+XS"><strong>Nexera XS</strong></a> inert LC and Shim-pack Scepter Claris column using HFIP (hexafluoroisopropanol) and 10 mM TEA (triethylamine) as ion pair additives.&nbsp;</p><p><strong>Mass Spectrometry Detection. </strong>Shimadzu Single Quadrupole<a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=+LCMS-2050"><strong> LCMS-2050</strong></a>. Data acquired in profile mode. MS mass scan m/z 600-2000; 1 secs; negative ion mode.</p><h4><strong>3.Results&nbsp;</strong></h4><h5><strong>3.1 Workflows and Methods&nbsp;</strong></h5><p>Insight Biologics software application supports two workflows to help accelerate oligonucleotide characterization. The default data processing behavior was driven by a defined FLP sequence to confirm sequence composition, identify product related impurities and assess impurity profiles. Data processing has been further augmented by enabling automated deconvolution routines to be applied without a defined FLP sequence input to help workflows that need to quickly check on molecular mass information in a synthesis (Figure 2).</p><h4><strong>4. Conclusions&nbsp;</strong></h4><ul><li>LabSolutions Insight Biologics offers flexibility by supporting both user-defined and automated deconvolution workflows for comprehensive oligonucleotide analysis.&nbsp;</li><li>A Quick Picking algorithm has been developed and applied to the analysis of 20-mer and 80-mer antisense DNA. In the case of a 20-mer sample, the FLP and associated impurities were also automatically detected and molecular weight information reported. The analysis showed high correspondence with data processing results using a defined FLP sequence input.&nbsp;</li><li>The Quick Picking algorithm enables a molecular weight confirmation of any detected peak and can be a powerful tool for synthesis confirmation in cases where the product is not as intended.&nbsp;</li><li>This LC-MS analysis platform provides a rapid and cost-effective solution for purity analysis and molecular weight confirmation, making it ideal for quality control environments.</li></ul><h3><strong>3. Thermo Fisher Scientific / ASMS: Comprehensive data acquisition workflow on a modified Orbitrap Astral MS to achieve deep lipidome coverage with high confidence annotations</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_003964_ms_ASMS_25_Astral_Zoom_Lipidomics_po003964_na_en_0ccd4bd053.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Lipid identification is often considered the most challenging and bottleneck of the lipidomics workflow. This is due to the vast diversity of lipid structures, isomers and varying concentrations. Fragmentation of lipids generate characteristic fragments that help in lipid annotation, structural elucidation, isomer differentiation, and improved confidence in lipid identification. Having fragmentation for most of the lipids detected in a sample hence is highly desirable. This requires fast and sensitive instrumentation. Here we evaluated the new Orbitrap Astral Zoom mass spectrometer (Figure 1) for deeper lipidome coverage and confident lipid identification from 73 mice plasma extracts.</p><h4><strong>Materials and methods&nbsp;</strong></h4><h5><strong>Sample Preparation&nbsp;</strong></h5><p>Lipids were extracted from plasma samples obtained from 73 mice fed with a high fat diet and a normal diet. Lipid standards and bovine liver lipid extracts were purchased from Avanti Polar Lipids.&nbsp;</p><h5><strong>LCMS Method&nbsp;</strong></h5><p>Plasma lipid extract was separated using Thermo Scientific nanoLC PepMap (C18, 75µmx150mm, 2µm) column connected to a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC system</strong></a>. Data acquisition was carried out on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom mass spectrometer</strong></a> using full-scan Orbitrap MS1 in parallel with data-dependent Astral MS2.</p><h5><strong>Data Analysis&nbsp;</strong></h5><p>Data processing was performed using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1759"><strong>Thermo Scientific Compound Discoverer 3.4 software</strong></a>. Compound Discoverer 3.4 software includes new features such as Thermo Scientific LipidSearch software node for simplified lipid identification, QC for small molecule experiments using internal standards, automatically detects and groups MS1 fragments and other performance improvements.</p><h4><strong>Results&nbsp;</strong></h4><h5><strong>Orbitrap Astral Zoom mass spectrometer DDA MS2 scan rate&nbsp;</strong></h5><p>The Orbitrap Astral Zoom mass spectrometer offers an enhanced MS2 scan rate compared to the already high-speed Orbitrap Astral MS system, enabling DDA with Top 30, Top 40, or even Top 50 MS2 scans (Figure 2) without compromising data quality. This advancement delivers unprecedented speed, achieving faster DDA MS2 scan rates than ever before.</p><h5><strong>Unprecedented speed and depth: dual analyzer power of Orbitrap Astral Zoom MS</strong></h5><p>The parallel data acquisition on Orbitrap Astral Zoom MS using both the Thermo Scientific Orbitrap analyzer and Thermo Scientific Astral analyzer, enables a higher number of Orbitrap HRAM MS1 full scans with sub-ppm mass accuracy. Simultaneously, the fast Astral analyzer delivers a significantly greater number of highquality MS2 scans at 80k resolution (77% more) compared to Orbitrap-Orbitrap configurations, which is essential for deep coverage and confident lipid identification (Figure 3).</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>The novel Orbitrap Astral Zoom mass spectrometer provides deeper lipidome coverage and confident identification, utilizing the parallel operation of Orbitrap and Astral analyzers.&nbsp;</li><li>The enhanced MS2 speed in Orbitrap Astral Zoom mode, coupled with Stepped NCE, enables efficient data acquisition and comprehensive lipidome coverage with a 15% increase with grade A and B lipid annotation.&nbsp;</li><li>The use of nano-flow increased the sensitivity and the number of detected lipids while achieving a significant reduction in the use of sample and solvent.&nbsp;</li><li>A significant difference was observed between control and high fat diet mice samples with potential biomarker upregulated neutral lipids (triglycerides and cholesterol esters) in the high fat diet.</li></ul><h3><strong>4. Waters Corporation / ASMS: Routine EPA 1633 PFAS Analysis with a Novel Slotted Bandpass Ion Guide to Improve Signal Response Robustness</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008888_65b495feb8.pdf"><strong>Full PDF for download</strong></a></li></ul><p>With increasing regulatory pressure around PFAS monitoring, this study evaluates a robust and long-term solution for EPA 1633A-compliant PFAS analysis. It focuses on how the StepWave XR ion guide, integrated into the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=5&amp;search=Xevo+TQ+Absolute+XR"><strong>Waters Xevo TQ Absolute XR tandem quadrupole mass spectrometer,</strong></a> improves signal robustness and method stability across demanding environmental matrices such as river water, biosolids, and landfill leachate.</p><h4><strong>Materials and Methods</strong></h4><p>Samples included NIST-certified biosolids, landfill leachate, and spiked river water. Solid-phase extraction (SPE) was followed by LC-MS/MS analysis on an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier System</strong></a> with BEH C18 columns and detection via the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=5&amp;search=Xevo+TQ+Absolute+XR"><strong>Xevo TQ Absolute XR</strong></a> using negative electrospray ionization and MRM. The robustness of the method was assessed over 12 weeks with over 9,000 injections and weekly calibrations, using <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1544"><strong>waters_connect for Quantitation Software</strong></a> for data processing and review.</p><h4><strong>Results</strong></h4><p>Throughout the 12-week study, all sample types showed high consistency and low variability. For example, L-PFHxS in biosolids averaged 8.78 µg/kg (%RSD 7.2%) compared to the certified 9.39 µg/kg, while PFOA in landfill leachate showed a mean of 2.52 ng/mL (%RSD 2.7%). QC plots confirmed that all monitored PFAS met trueness and ion ratio targets across thousands of injections with no unscheduled downtime, highlighting the system’s long-term reliability.</p><h4><strong>Conclusion</strong></h4><p>The StepWave XR ion guide enabled reliable, high-throughput PFAS analysis with minimal maintenance and excellent reproducibility. The Xevo TQ Absolute XR maintained calibration stability, accurate quantitation, and strong matrix resilience across diverse sample types. Combined with streamlined software workflows, this setup is well-suited for routine EPA 1633A PFAS analysis in environmental labs.</p>

News from LabRulezLCMS Library - Week 27, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 14th July 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, Thermo Fisher Scientific / ASMS </strong>and<strong> Waters Corporation / ASMS!</strong></p><h3><strong>1. Agilent Technologies / ASMS: Faster Than the Speed of Life: A Rapid Screening Method for Select PFAS Compounds in Serum by RapidFire-MS</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_rapidfire_ms_pfas_serum_asms_2025_wp_243_en_agilent_c8b56f4dd5.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) are a broad class of compounds with a high degree of fluorination used in a variety of industries and consumer products over the past seventy years. Because of their widespread use, as well as their persistence and poorly understood effects on the human body, laboratories have started to monitor their presence in biological fluids, including serum. Biological samples are commonly prepared with protein precipitation. Additional cleanup steps such as solid phase extraction (SPE) with either C18 or weak anion exchange (WAX) sorbent can be used for increased sensitivity and cleanup. Alternatively, a pass-through cleanup using Captiva EMR-Lipid removes proteins and phospholipids through filtration, which significantly reduces sample complexity.</p><h4><strong>Experimental</strong></h4><p>Purchased serum was aliquoted into two sets of samples, one for protein precipitation (ppt) only and one for a protein precipitation plus Captiva EMR-Lipid based cleanup. For each preparation, 100 µL serum was aliquoted into a tube and spiked with 25 native and extracted isotopically labeled (EIS) compounds (EPA 533 list). The samples were vortexed for 1 minute and then crashed with 1% formic acid in cold ACN. They were vortexed for 3 minutes and then spun for 10 minutes to complete the crash. Samples undergoing the Captiva-EMR Lipid cleanup were then loaded onto a pre-rinsed cartridge and allowed to filter through (Figure 1). All samples were then spiked with the additional non-extracted isotopically labelled (NIS) compounds, vortexed, and transferred to a plate for analysis.</p><p>The RF/TQ system consisted of a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=RapidFire+400"><strong>RapidFire 400</strong></a> front end with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=1&amp;search=6495D+triple+quadrupole"><strong>6495D triple quadrupole mass spectrometer</strong></a> for detection. Samples were introduced into the mass spectrometer using a RapidFire cartridge for additional cleanup, and the total cycle time was about 12.5 seconds, with analytes detected in negative polarity. Specific method conditions are detailed in Tables 1 (RF) and 2 (MS).</p><h4><strong>Results and Discussion</strong></h4><h5><strong>Early Development Work&nbsp;</strong></h5><p>Feasibility studies for detection of PFAS compounds in serum using the RapidFire started by looking for PFAS background in the instrument and in all steps of the workflow. Early testing demonstrated no detectable background from any stage of the process.</p><p>RapidFire method development tested a variety of cartridges for optimal binding of the PFAS compounds, as well as determining the best state times and solvent conditions. For the preliminary work, the C18 cartridge appeared to have the best results, while the optimized elution solvent was 5 mM ammonium acetate in methanol.</p><p>Early experiments were performed to understand the effects of dilution and sample prep on the overall sensitivity of the method. When only a protein precipitation preparation was employed, dilution had a significant positive effect on analyte sensitivity, as shown in Figure 2. However, when the sample prep routine utilized protein precipitation in combination with a Captiva EMR-Lipid cleanup, additional dilution was not necessary and in fact decreased overall sensitivity, as shown in Figure 3. This is attributed to the removal of extraneous matrix using the Captiva EMR-Lipid device, which has a unique selectivity for unbranched alkane chains, capturing phospholipids while allowing PFAS compounds to pass through the sorbent bed unretained.</p><h5><strong>Custom Cartridge Work&nbsp;</strong></h5><p>This preliminary work was done using the C18 cartridge, but the cartridge had poor retention of the short-chain PFAS compounds (C5 and below). To address this issue, a cartridge was custom-packed with mixed mode material that included C18 and anion exchange resins. Further testing and method optimization for this specific packing material yielded better results across the board, but especially for the short-chain PFAS compounds. Sensitivity for most analytes was at or below 0.1 ppb, as summarized in Table 3, with a calibration range of 0.01- 10 ppb tested for all analytes.</p><h4><strong>Conclusions</strong></h4><ul><li>LOQs for most PFAS analytes of interest in serum were 0.1 ppb or below</li><li>Samples were injected every 12 seconds, allowing for high throughput analysis</li><li>Custom mixed mode cartridge had best overall performance&nbsp;</li><li>There was no background PFAS contribution from the RapidFire system</li></ul><h3><strong>2. Shimadzu / ASMS: Benchtop Matrix Assisted Laser Desorption Ionization Mass Spectrometry of PFAS for preliminary screening of environmental samples</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_2025_MP_588_4c415fced0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Per- and polyfluoroalkyl substances (PFAS) are persistent environmental contaminants which negatively impact human health and the environment.&nbsp;<br>High concentrations of PFAS in test samples can cause contamination of sensitive LC-MS/MS instruments requiring extensive decontamination procedures, resulting in significant downtime and costly delays in sample processing.&nbsp;</p><p>We present the development of a simple, cost-effective method for the rapid screening of PFAS samples using an entry-level linear benchtop MALDI-TOF mass spectrometer to identify samples containing high levels before they enter the analytical workflow.</p><h4><strong>Methods</strong></h4><p>PFOA and PFOS standards were purchased from Merck, UK. Stock solutions (1 ppm prepared in acetonitrile) were diluted in water to the required concentrations.&nbsp;</p><p>Samples were tested with a variety of MALDI matrices (CHCA, DHB, DHAP, DAN, NRM and TMGN), with norharmane (NRM) and 1,8-bis(tetramethylguanidino)-naphthalene (TMGN) identified for further investigation. Diluted samples were mixed with NRM (1 mg/mL) or TMGN (5 mg/mL) in 70:30 Acetonitrile:Water. Blank samples of UHP water were prepared to ensure no contamination was present. 1 µL of the mixture was spotted onto a FlexiMassSR48 slide and the samples were analysed using a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?manufacturerItems=3&amp;search=MALDI-8030"><strong>MALDI-8030 MALDI-TOF mass spectrometer</strong></a> (Shimadzu). Analysis conditions are shown in Fig 1. Peaks at m/z 314.2 and m/z 499.2 were monitored for PFOA and PFOS, respectively. 13C8PFOS (m/z 507) was used as an internal standard for PFOS samples with a final sample concentration of 6.25 ng/mL (see Fig. 2). MALDI-MSI was used to assess spot homogeneity and limits of detection were established.</p><p>Subsequently, PFHxA and PFBS standards were purchased from Merck, UK and analysed using the same method</p><h4><strong>Conclusion</strong></h4><ul><li>We have shown, in principle, that it is possible to use MALDITOF mass spectrometry to implement a simple pre-screening method for aqueous samples to prevent widespread contamination in a PFAS monitoring laboratory. Using just a 200 µL sample and minimal preparation, a full slide of samples can be acquired in less than 15 minutes&nbsp;</li><li>Spot imaging during method development highlighted the differences in homogeneity of PFOS and PFOA spots suggesting that multiple internal standards would be necessary to pursue semi-quantitative analysis.&nbsp;</li><li>Whole slide imaging can provide quick results for multiple samples across a range of PFAS concentrations in a single run with easy visual identification of potentially problematic samples.&nbsp;</li><li>As a linear MALDI-TOF method, these results do not confirm the presence of PFAS but may be used as an indicative result to modify further testing protocols. Confirmatory LC-MS/MS analysis is required to determine the presence and concentration of any PFAS.</li></ul><h3><strong>3. Thermo Fisher Scientific / ASMS: Enhanced resolution with multi-pass mode on the Orbitrap Astral Zoom mass spectrometer&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/PO_319_ms_ASMS_25_Astral_Zoom_TMT_po319_na_en_a16d57e473.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The introduction of Thermo Scientific TMT 32-plex, with reporter ions clustered into quadruplets spaced by 3 mDa, demands a resolving power of approximately 90 k at low m/z, which challenges state-of-the-art time-of-flight mass analyzers. The Thermo Scientific Orbitrap Astral mass spectrometer [1] typically achieves around 60 k resolution at m/z = 138, falling to 50 k under high space charge influence.&nbsp;</p><p>Here we present an enhanced resolution multi-pass method implemented in the new Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom mass spectrometer</strong></a> [2], significantly improving the resolving power at low m/z enabling TMT 32-plex on the Thermo Scientific Astral analyzer. The ions are repeatedly guided through a switchable prism deflector to extend the ion path while the principal aberrations are compensated, thereby more than doubling the resolution.</p><h4><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>The Orbitrap Astral Zoom Mass Spectrometer</strong></a></h4><p>The Orbitrap Astral Zoom mass spectrometer incorporates a range of novel technologies for higher speed, sensitivity, dynamic range and resolving power. A faster ion filter and quadrupole switching in combination with improved ion transfer times in the ion-routing multipole (IRM) and ion processor allow DIA methods (Thermo Scientific Pierce FlexMix calibration solution, 2 Th isolation window, 350-980 m/z range, Thermo Scientific Orbitrap MS and Astral MS/MS) with scan rates faster than 270 Hz (DDA methods &gt; 180 Hz). A duty cycle of up to 80 % at 270 Hz is made possible by a new accumulation stage in the bent trap (linear to 106 ions) which increases the effective ion injection into the IRM by up to 40 % (additional ~0.75 ms on top of 2 ms IT in a DIA method). Furthermore, an additional mode of the high-dynamic range detector of the Astral analyzer for low-input sample applications like single-cell proteomics boosts the single ion detection efficiency by about 10 % and thereby the sensitivity. In combination with a new peak deconvolution algorithm for enhanced spectral processing, this increases the depth of analysis. In addition, modified IRM hardware allows for faster stepped collision energy experiments for deeper spectral coverage (2 CE: 80 Hz (OT Astral), 180 Hz (Orbitrap Astral Zoom MS), 3 CE: 60 Hz, 150 Hz). A modified AGC filling in the Orbitrap by a new enhanced dynamic range mode (EDR) provides additional spectral complexity and sensitivity. Here, multiplexed ion injections with different accumulation times are used for different mass ranges taking the variation in signal intensity into account. In addition, the Astral analyzer incorporates a new multi-pass mode which enhances the resolving power for small masses by more than a factor of two, enabling TMT 32-plex measurement in the Astral analyzer.</p><h4><strong>Conclusions&nbsp;</strong></h4><p>The TMT HR Mode advances the capabilities of the Astral analyzer. Fast electronic switching of the relay prism opens an ion trap and guides the ions after three times their normal flight distance to the detector. This greatly boosts the resolving power, especially for small m/z ratios, thereby enabling baseline-resolved quadruplets of reporter ions in a TMT 32-plex sample. First results show a peak resolution well above 100 k while maintaining high mass accuracy and shot-to-shot stability. The TMT HR Mode is utilized within a novel acquisition scheme delivering greater throughput for protein identification and quantitation for multiplexing up to 32 samples. Achieving a throughput of over 440 samples per day, the proteome coverage included 4,299 quantified protein groups and 22,146 peptides.</p><h3><strong>4. Waters Corporation / ASMS: Assessing the Impact of Part-per-Billion Mass Accuracy Upon Forensic Toxicology Data-Independent Analysis Screening&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008882_68ab66ac31.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This poster presents a forensic toxicology screening approach using <strong>ultra-high mass accuracy</strong> to improve specificity and efficiency in the analysis of complex biological matrices, such as urine. The need for rapid, accurate, and cost-effective screening is critical in forensic laboratories. The study evaluates the impact of <strong>parts-per-billion (ppb) mass accuracy</strong> using the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1148"><strong>Waters Xevo MRT Mass Spectrometer</strong></a><strong> </strong>compared to previous DIA methods.</p><p>The method involved analyzing a commercial standard and ten anonymized urine samples, diluted and analyzed via the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/199"><strong>ACQUITY UPLC I-Class FTN PLUS System</strong></a> coupled with the <strong>Xevo MRT MS</strong>. Data acquisition was performed in <strong>MSE mode</strong> (data-independent acquisition) under positive electrospray ionization (ESI+) using a 15-minute gradient. Data were processed in waters_connect software, leveraging a comprehensive spectral library with over 2000 compounds.</p><p>Results demonstrated a <strong>root mean square (RMS) mass error of just 571 ppb</strong> for precursor ions, with 94% of compounds detected within 1 ppm, and 96% of fragment ions within the same tolerance. A key example illustrated how reducing fragment ion tolerance from 2 mDa to 0.2 mDa eliminated a false positive (Anabasine), correctly identifying Nicotine as the true analyte, showing how ppb-level accuracy increases identification confidence and minimizes misidentifications.</p><p>The study concludes that ppb mass accuracy significantly reduces false positives, lowers review workloads, and facilitates independent analysis by less experienced personnel. Additionally, it supports cost savings by minimizing the need for confirmatory testing, potentially reducing both financial and environmental burdens in forensic laboratories.</p>

News from LabRulezLCMS Library - Week 29, 2025

<p><strong>Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 21st July 2025? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!</strong></p><blockquote><p><span style="font-size:20px;">👉 </span><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library"><span style="font-size:20px;"><strong>SEARCH THE LARGEST REPOSITORY OF DOCUMENTS ABOUT LCMS AND RELATED TECHNIQUES</strong></span></a></p></blockquote><blockquote><p><strong>👉 Need info about different analytical techniques?</strong> Peek into <a target="_blank" rel="noopener noreferrer" href="https://gcms.labrulez.com/library"><strong>LabRulezGCMS</strong></a> or <a target="_blank" rel="noopener noreferrer" href="https://icpms.labrulez.com/library"><strong>LabRulezICPMS</strong></a> libraries.</p></blockquote><p>This week we bring you posters by <strong>Agilent Technologies / ASMS, Shimadzu / ASMS, Thermo Fisher Scientific / ASMS, Waters Corporation / ASMS</strong> and application note by<strong> Metrohm!</strong></p><h3><strong>1. Agilent Technologies / ASMS: De Novo PFAS Annotation and Classification Using Highly Accurate Formula Prediction and Kaufmann Algorithms Embedded in FluoroMatchSuite</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ps_fluoromatch_de_novo_pfas_annotation_asms_2025_wp_113_en_agilent_4190191ba4.pdf"><strong>Full PDF for download</strong></a></li></ul><p><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=10&amp;search=FluoroMatch+Suite"><strong>FluoroMatch Suite </strong></a><strong>MS1 Only Algorithms: </strong>FluoroMatch Suite covers the entire non-targeted PFAS workflow (Figure 1) using MS/MS algorithms and the largest fragmentation database to date providing a &lt;5% false positive rate. However, MS/MS coverage is often incomplete, and DIA methods often provide lower quality spectra after deconvolution. Therefore, we developed MS1 only algorithms for providing highly accurate formula predictions (Figure 2) and for classifying features as PFAS or not PFAS using Kaufmann analysis (Figure 3)&nbsp;</p><p><strong>Validation: </strong>Algorithms were validated on NIST A and NIST C samples from the NIST PFAS interlaboratory study. NIST A consisted of known PFAS chemical standards, and NIST C consisted of an aqueous fire fighting foam (AFFF) contaminated soil sample. Formula prediction with homologous series voting (taking the most common repeating formula) was extremely accurate for both samples with a 0% false positive rate, and without homologous series voting the false positive rate was between 17-26% (Table 1). Kaufmann Analysis was highly specific for classifying PFAS with only 4% of non-PFAS being classified as PFAS with our Kaufmann based model, and only 6% of PFAS not be classified as PFAS according to our model for NIST C (Table 2).</p><h3><strong>2. Metrohm: Detection of heavy metals with differential pulse voltammetry</strong></h3><ul><li>Application note</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_sens_002_download_aa3cc76472.pdf"><strong>Full PDF for download</strong></a></li></ul><p>DPV, alongside square wave voltammetry (SWV), already discussed in <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/an_sens_001_download_6ed955a5ff.pdf"><strong>AN-SENS-001</strong></a>, is another example of a pulsed voltammetric technique. DPV was actually developed first and is often linked to the field of polarography. This pulsed voltammetric technique is typically used with a dropping mercury electrode, although the general principle can be applied to static electrodes as well. In the case of DPV, a short pulse with constant height is superimposed at the end of every step of a staircase linear sweep voltammetry (LSV) determination (Figure 1). During the experiment, the current is sampled at two points: before (i1 ) and after (i2 ) the pulse. The difference (i1 -i2 ) vs. the potential is the signal which is plotted in DPV. Sometimes i1 is referred to as the base current and i2 as the pulse current. Figure 1. Typical DPV waveform for the forward direction (e.g., from 0 to 1 V).&nbsp;</p><p>Like SWV, this approach allows the separation of faradaic and capacitive current, boosting the sensitivity of the technique compared to normal staircase voltammetry. In <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=INTELLO"><strong>INTELLO</strong></a>, the i1 and i2 signals can optionally be sampled in the signals tab of the DPV command. In NOVA, custom plots of either signal can be produced in the same tab. The waveform is characterized by the height of the pulse (ΔE) and the step height (ΔEs ). The scan rate is determined only by step height and step duration of the underlying LSV. The pulse duration should not be set longer than the step duration in order to avoid artifacts, with typical values for the step being around 100–500 ms, and around 50 ms for the pulse. In comparison to SWV, DPV is considered less applicable to a wider range of systems due to the interference of oxygen and the slower scan rates required for DPV. In some cases it can produce better separation of closely positioned peaks and sharper peaks in general. The following is an example of a typical DPV measurement made with a <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=PGSTAT302N"><strong>PGSTAT302N</strong></a> and the Metrohm 663 VA stand, with the same measurement also possible with the next-generation <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=220&amp;search=VIONIC"><strong>VIONIC </strong></a>powered by INTELLO.</p><h4><strong>SAMPLE AND EXPERIMENTAL DETAILS&nbsp;</strong></h4><p>A PGSTAT302N equipped with a Metrohm 663 VA stand (2.663.0020) was used for this study. The working electrode (WE) was a Multi-Mode Electrode pro (6.1246.120) in the hanging dropping mercury electrode (HDME) configuration. The reference electrode (RE) was a double junction Ag/AgCl reference electrode (6.0728.120). All potential values mentioned in this Application Note are referred to the potential of this electrode. The electrolyte was composed of 10 mL H2 O + 0.5 mL of acetate buffer, made of 1 mol/L ammonium acetate + 1 mol/L acetic acid.&nbsp;</p><p>The concentration of heavy metal ions was quantified by making two standard additions. For the first addition, the solution was composed as follows: 10 mL H2 O, 500 μL acetate buffer, 100 μL Pb standard solution (1 mg/L), and 100 μL Cd standard solution (1 mg/L). For the second addition, the solution was composed as follows: 10 mL H2 O, 500 μL acetate buffer, 200 μL Pb standard solution (1 mg/L), and 200 μL Cd standard solution (1 mg/L).&nbsp;</p><p>Each measurement consisted of a step to precondition the Hg electrode, where nitrogen was purged in the stirring solution and a new Hg drop was formed. Then, a reduction potential of -0.9 V was applied at the Hg drop in order to reduce the Pb and Cd cations at the Hg drop surface under stirring conditions and accumulate them at the Hg drop. The stirrer was then switched off and the DPV measurement was performed by oxidizing the previously accumulated Pb and Cd in a positive potential sweep from -0.9 to -0.2 V. The DPV measurement was repeated twice.&nbsp;</p><p>The peak heights were determined from the current vs. potential plot of the three experimental iterations (i.e., sample, sample with first standard addition, and sample with second standard addition). Peak height vs. analyte concentration plots were created for both Pb and Cd. The analyte concentration in the sample can be calculated from the intersection of the regression line with the x-axis.</p><h3><strong>3. Shimadzu / ASMS: EPA 533 and 537.1 with the Novel LCMS-8050RX: Demonstration of Instrument and Method Performance to meet PFAS regulatory levels&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/ASMS_25_TP_270_ebf0e2c9b0.pdf"><strong>Full PDF for download</strong></a></li></ul><p>The harmful impacts of per- and polyfluorinated alkyl substances (PFAS) continue to afflict the environment. Water utilities require sensitive and robust analytical methods to assess the current and ongoing burden of PFAS from source waters to meet regulatory demands in treated water and to protect public health. Improvements in sensitivity and/or runtime without sacrificing robustness can aid laboratories by increasing sample throughput to better meet the significant demand for PFAS sample analysis. The novel RX probe was developed to yield better heat distribution and more consistent nebulization to improve sensitivity and reproducibility. Chromatographic improvements compared to existing EPA methods were also performed to decrease runtime while maintaining the integrity of sample analysis.</p><h4><strong>Methods</strong></h4><p>PFAS were separated by a Nexera LC and quantified by a Shimadzu <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/library?mainauthorItems=1&amp;search=LCMS-8050RX"><strong>LCMS-8050RX</strong></a> for EPA methods 533 and 537.1 (EPAM533 and EPAM537.1). Neat standards were analyzed in the required composition (i.e., 80% methanol for EPAM533 and 96% methanol for EPAM537.1). Standards were analyzed twenty times to determine the instrument detection limits.</p><h4><strong>Results and Conclusion</strong></h4><ul><li>All PFAS were sufficiently analyzed by the respective methods and passed regulatory criteria at a reduced runtime (19 minutes shorter).</li><li>Superb precision and reproducibility were demonstrated with the RX probe, which resulted in an analytical blueprint that greatly exceeds the Final PFAS National Primary Drinking Water Regulation promulgated in 2024.</li></ul><h3><strong>4. Thermo Fisher Scientific / ASMS: Comprehensive and high-throughput plasma proteome profiling for biomarker discovery using the Orbitrap Astral Zoom Mass Spectrometer and the Seer Proteograph ONE workflow</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/po_381_plasma_proteome_profiling_biomarker_discovery_po381_asms2025_en_074e0d2a50.pdf"><strong>Full PDF for download</strong></a></li></ul><p>Plasma proteomics, the study of proteins in blood plasma, is crucial for biomarker discovery and understanding global signaling and immune responses1, aiding disease diagnosis, monitoring, and personalized medicine. However, the plasma proteome's complexity and dynamic range—spanning up to 12 orders of magnitude²—pose challenges, especially for detecting low-abundance proteins. Additionally, preanalytical, analytical, and biological variables complicate reliable biomarker identification, necessitating optimized techniques³. Liquid chromatography-mass spectrometry (LC-MS) excels in plasma proteomics due to its high analytical dynamic range and capability to measure peptides and characterize posttranslational modifications (PTMs). Advances in sample preparation, separation, MS, and data analysis are improving method sensitivity and robustness. We demonstrate the Thermo ScientificTM OrbitrapTM AstralTM Zoom Mass Spectrometer's high sensitivity and reproducibility in detecting a comprehensive plasma proteome across neat, depleted, and plasma processed with the Seer® Proteograph® ONE workflow, facilitating potential biomarker discovery¹.</p><h4><strong>Experimental Procedure</strong></h4><h5><strong>Liquid chromatography-mass spectrometry &amp; data analysis</strong></h5><p>All LC-MS runs for neat, depleted, and Proteograph ONE processed peptides were separated and analyzed using a Thermo Scientific <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC</strong></a> System in trap and elute configuration, paired with an <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/1959"><strong>Orbitrap Astral Zoom Mass Spectrometer</strong></a>. Peptides were separated on the <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/398"><strong>Vanquish Neo UHPLC</strong></a> System using Thermo Scientific EASY-Spray PepMap analytical columns (ES906, 2µm C18, 150µm × 15 cm for 100 and 60 SPD and ES75500PN 2µm C18, 75µm × 50 cm for 24SPD) and 12.6-, 22.35-, and 54-minute chromatographic gradients, respectively, were formed using 0.1% formic acid in water for mobile phase A and 0.1% formic acid in 80% acetonitrile for mobile phase B. Samples were injected with 2 loading mass amounts (200/500 ng for 100/60 SPD; 500/1250 ng for 24 SPD) in triplicate. Liquid chromatography parameters are shown below in Table 1A. Mass spectrometer scan parameters can be found below in Table 1B. All data was processed using the Proteograph® Analysis Suite (PAS) (Seer). Output files were imported to Rstudio (2023.09.0 Build 463) with R (v4.3.1) for downstream data analysis and visualization.</p><h4><strong>Conclusions&nbsp;</strong></h4><ul><li>With the Orbitrap Astral Zoom Mass Spectrometer, neat plasma proteome coverage exceeds 1,000 protein groups in a single pooled sample, providing exceptional quantitative precision without additional sample handling steps.&nbsp;</li><li>High Select Top 14 abundant protein depletion enhances plasma proteome depth by ~2x across 100, 60, and 24 SPD throughputs with comparable or superior analytical measurement precision.&nbsp;</li><li>Seer Proteograph ONE enhances plasma proteome depth by 7.9x (100SPD), 6.9x (60SPD), and 6.2x (24SPD) with comparable or superior analytical measurement precision and no compromise on sample preparation throughput.&nbsp;</li><li>The combination of the Orbitrap Astral Zoom Mass Spectrometer and the Proteograph ONE Workflow allows for over 7,000 protein groups to be identified from a single injection.&nbsp;</li><li>The speed, sensitivity, and robustness of the Orbitrap Astral Zoom Mass Spectrometer enables in-depth biological discovery, paving the way for novel findings and advancements in clinical cohort and population-scale translational research.</li></ul><h3><strong>5. Waters Corporation / ASMS: PFASt and Furious: A Targeted and Non-Targeted LC-MS/MS Study on the Environmental Impact of Using Fluorinated Ski Waxes&nbsp;</strong></h3><ul><li>Poster</li><li><a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/labrulez-bucket-strapi-h3hsga3/720008880_8590308c24.pdf"><strong>Full PDF for download</strong></a></li></ul><p>This study by Waters Corporation explores the environmental impact of fluorinated ski waxes—specifically per- and polyfluoroalkyl substances (PFAS)—on soil and water quality at competitive ski sites in New England. Using both targeted LC-MS/MS and non-targeted high-resolution mass spectrometry, the research team analyzed samples from slalom and cross-country racing courses to determine the extent of PFAS contamination.</p><p>PFAS were found in all collected samples, with soil showing significantly higher concentrations than water. Long-chain perfluorocarboxylic acids, commonly used in ski waxes, dominated the contaminant profile. At slalom courses, the highest concentrations were found at the wax application zones near the start line, decreasing progressively downhill. At cross-country sites, similar patterns emerged near waxing and testing areas, with alarming migration of PFAS into adjacent ponds and even a vegetable garden.</p><p>The study employed automated sample preparation systems (CEM EDGE and Promochrom SPE-03) to ensure efficiency and reproducibility. Advanced LC-MS/MS analysis with Waters’ <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/191"><strong>ACQUITY Premier </strong></a>and <a target="_blank" rel="noopener noreferrer" href="https://lcms.labrulez.com/products/554"><strong>Xevo TQ Absolute</strong></a> platforms enabled the detection of common PFAS, while cyclic ion mobility HRMS revealed additional, untargeted long-chain species (e.g., C15/C16 carboxylic acids) not typically included in regulatory workflows.</p><p>The findings highlight the long-term environmental risks posed by legacy ski wax formulations and underscore the need for continued monitoring. Notably, unexpected PFOS levels in garden soil suggest multiple PFAS sources may be contributing to contamination, warranting further investigation.</p>

News from LabRulezLCMS Library - Week 30, 2025

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News from LabRulezLCMS Library - Week 31, 2025

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